CN113693994A - White mulberry root-bark extract with whitening and bacteriostasis functions as well as preparation method and application thereof - Google Patents
White mulberry root-bark extract with whitening and bacteriostasis functions as well as preparation method and application thereof Download PDFInfo
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- CN113693994A CN113693994A CN202111210593.0A CN202111210593A CN113693994A CN 113693994 A CN113693994 A CN 113693994A CN 202111210593 A CN202111210593 A CN 202111210593A CN 113693994 A CN113693994 A CN 113693994A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9789—Magnoliopsida [dicotyledons]
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P17/00—Drugs for dermatological disorders
- A61P17/10—Anti-acne agents
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P31/00—Antiinfectives, i.e. antibiotics, antiseptics, chemotherapeutics
- A61P31/04—Antibacterial agents
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q17/00—Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
- A61Q17/005—Antimicrobial preparations
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/02—Preparations for care of the skin for chemically bleaching or whitening the skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/52—Stabilizers
- A61K2800/524—Preservatives
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/81—Preparation or application process involves irradiation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
The invention discloses a preparation method of a cortex mori extract, which comprises the following steps: the method comprises the following steps: extracting cortex Mori with ethanol to obtain cortex Mori extract, decolorizing, and filtering to obtain cortex Mori filtrate; step two: sequentially carrying out primary molecular distillation and secondary molecular distillation on the cortex mori radicis filtrate, and merging light fractions obtained by molecular distillation to obtain cortex mori radicis molecular distillate; step three: vacuum filtering cortex Mori molecular distillate with diatomaceous earth cake, extracting with ethanol twice to obtain cortex Mori secondary ethanol extract, and rotary steaming and concentrating to obtain cortex Mori concentrate; step four: pretreating cortex Mori concentrate, vacuum filtering, adding 1, 3-propylene glycol, and compounding to obtain cortex Mori extract. The cortex mori extract prepared by the invention has good stability, can effectively lighten melanin in skin, effectively inhibit abnormal reproduction of propionibacterium acnes, has good antiseptic property, and can be used for preparing cosmetics with related effects.
Description
Technical Field
The invention relates to the technical field of cosmetics, in particular to a whitening and bacteriostatic cortex mori extract, a preparation method thereof and application thereof in cosmetics.
Background
Cortex mori is dry root bark of dicotyledonous plant mulberry after removal of embolus, and was originally recorded in Shennong's herbal Jing, and is considered to be sweet and cold in nature, belongs to lung and spleen channels in traditional Chinese medicine, and has the effects of relieving asthma, promoting urination, reducing blood sugar and blood pressure, resisting cancer, protecting liver and the like. Recently, as studies on chemical components and pharmacological activities of white mulberry root-bark have been intensively studied, people have made a deeper understanding of the main components of white mulberry root-bark, and found that white mulberry root-bark extract contains sanggenon C, which is a main component inhibiting the activity of TYR (tyrosinase), flavonoids having good antioxidant ability, and certain components inhibiting acne-related pathogenic bacteria. Therefore, people turn their eyes to applying the cortex mori radicis extract to other fields in life.
At present, the method for extracting effective components without structural change from plants can be divided into a physical extraction or extraction method, a chemical reagent soaking method and a biological fermentation method, and a water extraction method and an alcohol extraction method are mostly used in industrial production, the two methods are simple to operate and low in cost, are safe and environment-friendly, and can protect the structures of the effective components to the maximum extent, but the extraction process or conditions are not mild, or the extraction rate is not high, so that the biological activity of the extract is low, and the whitening and bacteriostasis effects can be rapidly lost on line.
Acne is a chronic inflammatory skin disease of pilosebaceous tissues, and factors causing acne occurrence may include androgen increase, propionibacterium acnes mass propagation, inflammatory lesions, immune disorders and the like. The pathogenic bacterium Propionibacterium acnes is a gram-positive bacterium and is a normal flora of the skin on the surface of a human body, but when the Propionibacterium acnes excessively proliferates, a large amount of enzyme containing biological activity is released to trigger the hyperplasia and excessive keratinization of a pilosebaceous canal, and meanwhile, inflammatory mediators are released to finally cause the generation of acne. The cortex Mori extract has effect in improving acne by inhibiting mass propagation of Propionibacterium acnes, and can be used for preparing skin care product for improving acne.
CN109078047B discloses a preparation method of a cortex mori extract, which comprises the steps of firstly extracting with ethanol and then carrying out macroporous resin chromatography; CN102836218A discloses a preparation method of a cortex mori radicis extract, which takes water as an extractant and adopts cellulase for extraction, filtration, reduced pressure concentration and freeze drying to obtain the cortex mori radicis product. However, the above method does not pay attention to the stability of the extract of cortex mori.
Therefore, the prior art does not provide a cortex mori extract with good stability and better whitening, antibacterial and preservative activities.
Disclosure of Invention
In order to solve the above problems, the invention aims to provide a preparation method of a cortex mori extract for whitening and bacteriostasis, which comprises the following steps:
the method comprises the following steps: heating and refluxing the cortex mori radicis by using ethanol with the mass concentration of 70-90% for 3-4 hours at the temperature of 70-90 ℃ for primary ethanol extraction to obtain a cortex mori radicis primary ethanol extract, decoloring and filtering to obtain a cortex mori radicis filtrate;
step two: sequentially carrying out primary molecular distillation and secondary molecular distillation on the cortex mori radicis filtrate, and merging light fractions obtained by molecular distillation to obtain cortex mori radicis molecular distillate;
step three: performing vacuum filtration on the cortex mori molecular distillate by using diatomite cake, performing secondary alcohol extraction to obtain a cortex mori secondary alcohol extract, and performing rotary evaporation and concentration to obtain a cortex mori concentrate;
step four: pretreating the cortex mori radicis concentrate, carrying out vacuum filtration, adding 1, 3-propylene glycol to compound to the full weight of the pretreated cortex mori radicis concentrate, and obtaining the cortex mori radicis extract.
Further, in the second step, the first-stage molecular distillation and the second-stage molecular distillation are carried out under the assistance of microwaves, the microwave power is 100-.
Preferably, the microwave extraction power is 150-250W, and the distillation extraction time is 50-90 min.
Further, in the second step, the conditions of the first-stage molecular distillation are as follows: the distillation pressure is 0.1-10 Pa, the sample injection temperature is 40-50 ℃, the distillation temperature is 50-80 ℃, the condensation temperature is 20-40 ℃, and the feeding speed is 10-1000 g/h;
the conditions of the secondary molecular distillation are as follows: the distillation pressure is 0.1-10 Pa, the injection port temperature is 50-70 ℃, the distillation temperature is 100-120 ℃, the condensation temperature is 60-70 ℃, and the feeding speed is 10-1000 g/h.
Preferably, the conditions of the primary molecular distillation are as follows: the distillation pressure is 0.1-5 Pa, the sample injection temperature is 40-45 ℃, the distillation temperature is 55-75 ℃, the condensation temperature is 25-35 ℃, and the feeding speed is 10-100 g/h;
the conditions of the secondary molecular distillation are as follows: the distillation pressure is 0.1-5 Pa, the injection port temperature is 50-65 ℃, the distillation temperature is 105-115 ℃, the condensation temperature is 62-68 ℃, and the feeding speed is 10-100 g/h.
More preferably, the conditions of the primary molecular distillation are as follows: the distillation pressure is 0.1-1 Pa, the sample introduction temperature is 41-43 ℃, the distillation temperature is 60-72 ℃, the condensation temperature is 28-32 ℃, and the feeding speed is 10-50 g/h;
the conditions of the secondary molecular distillation are as follows: the distillation pressure is 0.1-1 Pa, the injection port temperature is 50-60 ℃, the distillation temperature is 108-112 ℃, the condensation temperature is 63-66 ℃, and the feeding speed is 10-50 g/h.
Further, before alcohol extraction, mulberry bark powder is prepared in the step one: selecting clean and disease-free dry cortex mori radicis, and crushing.
Preferably, the grinding mesh number is 100-600 meshes.
Further, in the first step, the weight of the white mulberry root-bark is 500-600 g, the mass concentration of the ethanol is 75-85%, and the using amount of the ethanol is 6-10 times of the weight of the white mulberry root-bark.
Preferably, the ethanol accounts for 7-9 times of the mass of the cortex mori radicis powder.
Further, activated carbon is adopted for decoloring in the first step, and the specific steps are as follows: 100-120 g of activated carbon, and filtering to remove the activated carbon when the activated carbon is hot after the activated carbon is decolorized by heating in a water bath at 70-90 ℃ for 30-60 min.
Preferably, the decolorizing condition is that after heating in a water bath at 75-85 ℃ for 40-50 min, the active carbon is removed by filtering while the solution is hot.
Further, in the third step, the diatomite cake is prepared from diatomite and EDTA-2Na, the dosage of the diatomite is 1% -10% of the mass of the cortex mori radicis molecular distillate, the dosage of the EDTA-2Na is 0.2% -5% of the mass of the cortex mori radicis molecular distillate, and the dosage of pure water for eluting the filter cake is 250-1000 ml.
Preferably, the dosage of the diatomite is 3-5% of the mass of the filtered sample, the dosage of the EDTA disodium is 0.5-1% of the mass of the filtered sample, and the dosage of pure water for eluting the filter cake is 300-500 ml.
Further, before vacuum filtration in the third step, the cortex mori molecular distillate is cooled to 50-70 ℃; and/or
The secondary alcohol extraction adopts absolute ethyl alcohol as an extractant, and the heating reflux is carried out for 3 to 4 hours at the temperature of 70 to 90 ℃; and or (b) a,
the rotary evaporation concentration conditions are as follows: the vacuum degree is 100-200 mbar, and the water bath temperature is 70-80 ℃.
Further, the pretreatment of the cortex mori radicis concentrate in the fourth step comprises the steps of adding 25-30% of deionized water and 66-74% of 1, 3% of propylene glycol into 1-4% of the concentrate, fully dissolving, adding 5-8% of diatomite, stirring for 2-3 hours, and standing overnight.
Further, the processing of the cortex mori radicis concentrate in the fourth step comprises: after compounding, stirring until the mixture is clear and transparent.
Further, the sterilization and canning of the compounded cortex mori radicis concentrate in the fourth step comprises the following steps: sterilizing at 70-80 ℃ for 1-3 hours, cooling to 30-40 ℃, and canning.
On the other hand, the application also provides a cortex mori extract prepared by the preparation method.
On the other hand, the application also provides application of the white mulberry root-bark extract prepared by the preparation method of the white mulberry root-bark extract for whitening and inhibiting bacteria in preparation of a product for inhibiting growth of propionibacterium acnes and/or lightening skin melanin.
Preferably, the Propionibacterium acnes-growing and/or skin melanin lightening product includes, but is not limited to, cosmetics.
Alternatively, the cosmetic may be in the form of, but not limited to, aqueous, lotion, cream, essence, gel, etc.
Preferably, the concentration of the cortex mori radicis extract in the product is 0.025-50% v/v.
The invention has the beneficial effects that:
1. according to the application, the cortex mori radicis extract with high purity and no impurities is obtained through the step of performing molecular distillation on the cortex mori radicis alcohol extract when the ethanol is used for extracting the cortex mori radicis, and compared with the extract prepared by the traditional process, the extract has the advantages that the content of bioactive components for whitening and bacteriostasis and the effect of the bioactive components are remarkably improved, and further, the whitening and bacteriostasis effect can be better; meanwhile, the stability of the cortex mori radicis extract can be further improved by optimizing parameters in the molecular distillation step, so that the cortex mori radicis extract is more suitable for cosmetic raw materials.
2. The cortex mori extract prepared by the invention can effectively lighten melanin in skin, can effectively inhibit abnormal reproduction of propionibacterium acnes, has good antiseptic property, and can be used for preparing cosmetics with related effects.
The specific implementation mode is as follows:
in the following description, numerous specific details are set forth by way of examples in order to provide a more thorough understanding of the present invention. It will be apparent, however, to one skilled in the art, that the present invention may be practiced without one or more of these specific details. In other instances, well-known features have not been described in order to avoid obscuring the invention.
The materials and equipment used in the following examples are commercially available, and if not specifically mentioned, the raw material grades in the following examples are all cosmetic grades and are all commercially available.
In addition, the "water" in the present invention includes any available water that can be used in the cosmetic field such as deionized water, distilled water, ion-exchanged water, double distilled water, high purity water, purified water, and the like.
Example 1
The embodiment provides a preparation method of a cortex mori extract for cosmetics, which comprises the following specific steps:
firstly, selecting clean and disease-free dry cortex mori radicis, and crushing the dry cortex mori radicis with 400 meshes to obtain cortex mori radicis powder;
secondly, weighing 500g of cortex mori radicis powder, adding 4000g of ethanol with the mass concentration of 75% for primary ethanol extraction, heating and refluxing at the temperature of 90 ℃ for 3 hours to obtain a primary ethanol extract of the cortex mori radicis, adding 120g of activated carbon after the primary ethanol extract is obtained, uniformly stirring, placing the mixture in a water bath kettle at the temperature of 80 ℃ for water bath heating and decoloring for 60 minutes, and filtering to remove the activated carbon while the mixture is hot;
thirdly, sequentially carrying out primary molecular distillation and secondary molecular distillation on the cortex mori radicis filtrate under the assistance of microwaves, and combining light fractions obtained by the molecular distillation to obtain cortex mori radicis molecular distillate, wherein the microwave extraction power is 200W, and the distillation extraction time is 60 min;
the conditions of the first-stage molecular distillation are as follows: the distillation pressure is 0.1Pa, the sample injection temperature is 41 ℃, the distillation temperature is 68 ℃, the condensation temperature is 28 ℃ and the feeding speed is 10 g/h;
the conditions of the secondary molecular distillation are as follows: the distillation pressure is 0.1Pa, the injection port temperature is 50 ℃, the distillation temperature is 108 ℃, the condensation temperature is 63 ℃ and the feeding speed is 10 g/h;
fourthly, paving diatomite with 5% of the mass of the white mulberry root-bark molecular distillate and 1% of EDTA disodium in a beaker, adding pure water, uniformly stirring, carrying out vacuum filtration to obtain a diatomite filter cake, eluting the diatomite filter cake again by using 500ml of pure water, removing metal ions in the filter cake, and reducing the conductivity;
fifthly, cooling the filtrate obtained in the second step to 60 ℃, performing suction filtration on the diatomite filter cake, performing rotary evaporation concentration on the obtained filtrate under the conditions of a vacuum degree of 160mbar and a water bath at 75 ℃, performing secondary alcohol extraction on the obtained concentrated solution, and heating and refluxing for 3.5 hours at 80 ℃ by adopting absolute ethyl alcohol as an extractant; the conditions of rotary evaporation and concentration are as follows: vacuum degree of 150mbar, water bath temperature of 75 deg.C, adding 120g active carbon, stirring, placing in 80 deg.C water bath kettle, heating and decolorizing for 60min, filtering to remove active carbon, filtering the decolorized filtrate, and concentrating to obtain paste concentrate;
sixthly, weighing 2% of paste concentrate, adding 28% of deionized water and 70% of 1, 3-propylene glycol to fully dissolve the paste concentrate, adding 8% of diatomite, stirring for 2 hours, and standing overnight;
seventhly, preparing the diatomite cake again, wherein the method is the same as the third step;
and eighthly, performing suction filtration on the pretreated extracting solution by using diatomite cake, adding 1, 3-propylene glycol to supplement the total weight to obtain a compounded clear and transparent extracting solution, heating and sterilizing the mixed extracting solution for 2 hours at the temperature of 80 ℃, cooling the mixed extracting solution to the temperature of 40 ℃, and canning the mixed extracting solution.
Example 2
The embodiment provides a preparation method of a cortex mori extract for cosmetics, which comprises the following specific steps:
firstly, selecting clean and disease-free dry cortex mori radicis, and crushing the dry cortex mori radicis to obtain cortex mori radicis powder;
secondly, weighing 500g of cortex mori radicis powder, adding 5000g of ethanol with the mass concentration of 75% for primary ethanol extraction, heating and refluxing at the temperature of 70 ℃ for 4 hours to obtain a primary ethanol extract of the cortex mori radicis, adding 120g of activated carbon after the primary ethanol extract is obtained, uniformly stirring, placing the mixture in a water bath kettle at the temperature of 70 ℃ for water bath heating and decoloring for 45min, and filtering to remove the activated carbon while the mixture is hot;
thirdly, sequentially carrying out primary molecular distillation and secondary molecular distillation on the cortex mori radicis filtrate under the assistance of microwaves, and combining light fractions obtained by the molecular distillation to obtain cortex mori radicis molecular distillate, wherein the microwave extraction power is 100W, and the distillation extraction time is 50 min;
the conditions of the first-stage molecular distillation are as follows: the distillation pressure is 0.2Pa, the sample injection temperature is 42 ℃, the distillation temperature is 69 ℃, the condensation temperature is 29 ℃, and the feeding speed is 20 g/h;
the conditions of the secondary molecular distillation are as follows: the distillation pressure is 0.2Pa, the injection port temperature is 52 ℃, the distillation temperature is 109 ℃, the condensation temperature is 64 ℃ and the feeding speed is 20 g/h.
Fourthly, paving the diatomite with the mass of 2% of the white mulberry root-bark molecular distillate and 0.5% of EDTA disodium in a beaker, adding pure water, uniformly stirring, carrying out vacuum filtration to obtain a diatomite filter cake, eluting the diatomite filter cake again by 1000ml of pure water, removing metal ions in the filter cake, and reducing the conductivity;
fifthly, cooling the filtrate in the third step to 40 ℃, performing suction filtration on the diatomite filter cake, performing rotary evaporation concentration on the obtained filtrate under the conditions of a vacuum degree of 160mbar and a water bath kettle at 70 ℃, performing secondary alcohol extraction on the obtained concentrated solution, and heating and refluxing for 3 hours at 70 ℃ by adopting absolute ethyl alcohol as an extractant; the conditions of rotary evaporation and concentration are as follows: vacuum degree of 100mbar, water bath temperature of 70 deg.C, adding 120g of activated carbon, stirring, placing in 80 deg.C water bath kettle, heating in water bath for decolorizing for 60min, filtering to remove activated carbon, and vacuum filtering and concentrating the decolorized filtrate to obtain paste concentrate;
sixthly, weighing 1% of paste concentrate, adding 25% of deionized water and 74% of 1, 3-propylene glycol for full dissolution, adding 5% of diatomite, stirring for 4 hours, and standing overnight;
seventhly, preparing the diatomite cake again, wherein the method is the same as the third step;
and eighthly, performing suction filtration on the pretreated extracting solution by using diatomite cake, adding 1, 3-propylene glycol to supplement the total weight to obtain a compounded clear and transparent extracting solution, heating and sterilizing the mixed extracting solution for 1 hour at the temperature of 80 ℃, cooling the mixed extracting solution to the temperature of 40 ℃, and canning the mixed extracting solution.
Example 3
The embodiment provides a preparation method of a cortex mori extract for cosmetics, which comprises the following specific steps:
firstly, selecting clean and disease-free dry cortex mori radicis, and crushing the dry cortex mori radicis to obtain cortex mori radicis powder;
secondly, weighing 500g of cortex mori radicis powder, adding 3000g of ethanol with the mass concentration of 90% for primary ethanol extraction, heating and refluxing at the temperature of 80 ℃ for 3.5 hours to obtain a primary ethanol extract of the cortex mori radicis, adding 100g of activated carbon after the primary ethanol extract is extracted, uniformly stirring, placing the extract in a water bath kettle at the temperature of 90 ℃ for heating and decoloring for 30min, and filtering to remove the activated carbon while the extract is hot;
thirdly, sequentially carrying out primary molecular distillation and secondary molecular distillation on the cortex mori radicis filtrate under the assistance of microwaves, and combining light fractions obtained by the molecular distillation to obtain cortex mori radicis molecular distillate, wherein the microwave extraction power is 300W, and the distillation extraction time is 100 min;
the conditions of the first-stage molecular distillation are as follows: the distillation pressure is 0.5Pa, the sample injection temperature is 43 ℃, the distillation temperature is 70 ℃, the condensation temperature is 30 ℃, and the feeding speed is 30 g/h;
the conditions of the secondary molecular distillation are as follows: the distillation pressure is 0.5Pa, the injection port temperature is 55 ℃, the distillation temperature is 110 ℃, the condensation temperature is 65 ℃, and the feeding speed is 30 g/h;
fourthly, paving kieselguhr with the mass of 3% of the white mulberry root-bark molecular distillate and 2% of EDTA disodium in a beaker, adding pure water, uniformly stirring, performing vacuum filtration to obtain a kieselguhr filter cake, eluting the kieselguhr filter cake again by using 250ml of pure water, removing metal ions in the filter cake, and reducing the conductivity;
fifthly, cooling the filtrate obtained in the second step to 40 ℃, performing suction filtration on the diatomite filter cake, performing rotary evaporation concentration on the obtained filtrate under the conditions that the vacuum degree is 100mbar and the water bath is 80 ℃, performing secondary alcohol extraction on the obtained concentrated solution, and heating and refluxing for 4 hours at 90 ℃ by adopting absolute ethyl alcohol as an extractant; the conditions of rotary evaporation and concentration are as follows: vacuum degree of 200mbar, water bath temperature of 80 deg.C, adding 120g active carbon, stirring, placing in 80 deg.C water bath kettle, heating and decolorizing for 60min, filtering to remove active carbon, filtering the decolorized filtrate, and concentrating to obtain paste concentrate;
sixthly, weighing 4% of paste concentrate, adding 30% of deionized water and 66% of 1, 3-propylene glycol for full dissolution, adding 7% of diatomite, stirring for 3 hours, and standing overnight;
seventhly, preparing the diatomite cake again, wherein the method is the same as the third step;
and eighthly, performing suction filtration on the pretreated extracting solution by using diatomite cake, adding 1, 3-propylene glycol to supplement the total weight to obtain a compounded clear and transparent extracting solution, heating and sterilizing for 4 hours at the temperature of 70 ℃, cooling to 25 ℃, and canning.
Example 4
The embodiment provides a preparation method of a cortex mori extract for cosmetics, which comprises the following specific steps:
firstly, selecting clean and disease-free dry cortex mori radicis, and crushing the dry cortex mori radicis to obtain cortex mori radicis powder;
secondly, weighing 600g of cortex mori radicis powder, adding 5000g of ethanol with the mass concentration of 75% for primary ethanol extraction, heating and refluxing at the temperature of 70 ℃ for 4 hours to obtain a primary ethanol extract of the cortex mori radicis, adding 120g of activated carbon after the primary ethanol extract is obtained, uniformly stirring, placing the mixture in a water bath kettle at the temperature of 70 ℃ for water bath heating and decoloring for 45min, and filtering to remove the activated carbon while the mixture is hot;
thirdly, sequentially carrying out primary molecular distillation and secondary molecular distillation on the cortex mori radicis filtrate under the assistance of microwaves, and combining light fractions obtained by the molecular distillation to obtain cortex mori radicis molecular distillate, wherein the microwave extraction power is 100W, and the distillation extraction time is 40 min;
the conditions of the first-stage molecular distillation are as follows: the distillation pressure is 1Pa, the sample injection temperature is 43 ℃, the distillation temperature is 72 ℃, the condensation temperature is 32 ℃, and the feeding speed is 50 g/h;
the conditions of the secondary molecular distillation are as follows: the distillation pressure is 1Pa, the injection port temperature is 60 ℃, the distillation temperature is 112 ℃, the condensation temperature is 66 ℃, and the feeding speed is 50 g/h;
fourthly, paving the diatomite with the mass of 2% of the white mulberry root-bark molecular distillate and 0.5% of EDTA disodium in a beaker, adding pure water, uniformly stirring, carrying out vacuum filtration to obtain a diatomite filter cake, eluting the diatomite filter cake again by 1000ml of pure water, removing metal ions in the filter cake, and reducing the conductivity;
fifthly, cooling the filtrate obtained in the second step to 60 ℃, performing suction filtration on the diatomite filter cake, performing rotary evaporation concentration on the obtained filtrate under the conditions of a vacuum degree of 160mbar and a water bath at 75 ℃, performing secondary alcohol extraction on the obtained concentrated solution, and heating and refluxing for 3.5 hours at 80 ℃ by adopting absolute ethyl alcohol as an extractant; the conditions of rotary evaporation and concentration are as follows: vacuum degree of 150mbar, water bath temperature of 75 deg.C, adding 120g active carbon, stirring, placing in 80 deg.C water bath kettle, heating and decolorizing for 60min, filtering to remove active carbon, filtering the decolorized filtrate, and concentrating to obtain paste concentrate;
sixthly, weighing 4% of paste concentrate, adding 30% of deionized water and 66% of 1, 3-propylene glycol for full dissolution, adding 7% of diatomite, stirring for 3 hours, and standing overnight;
seventhly, preparing the diatomite cake again, wherein the method is the same as the third step;
and eighthly, performing suction filtration on the pretreated extracting solution by using diatomite cake, adding 1, 3-propylene glycol to supplement the total weight to obtain a compounded clear and transparent extracting solution, heating and sterilizing the mixed extracting solution for 2 hours at the temperature of 80 ℃, cooling the mixed extracting solution to the temperature of 40 ℃, and canning the mixed extracting solution.
Examples 5 to 8
Examples 5 to 8 were prepared in substantially the same manner as in example 1, except that the microwave time for the molecular distillation, the distillation temperature for the primary molecular distillation, and the distillation temperature for the secondary molecular distillation used in the third step were different, as shown in Table 1.
Comparative example 1
This comparative example is substantially the same as the preparation method of example 1 except that the third step is not performed and the cortex mori filtrate is directly vacuum filtered.
Comparative example 2
This comparative example is about the same as the preparation of example 1, except that no microwave assisted distillation was used in the third step.
The extract of cortex mori radicis obtained from the above examples and comparative examples was tested for MIC of minimum inhibitory concentration against propionibacterium acnes and storage stability under various environments. Wherein, the tested samples are all the original white mulberry root-bark extract without being prepared with 1, 3-propylene glycol and water after the solvent is removed; the test method for the minimum inhibitory concentration MIC of Propionibacterium acnes is described below; the endurance test time under different treatment environments is 72 h. The results are shown in Table 1.
TABLE 1
As can be seen from the data in Table 1, when the microwave distillation extraction time is 50-90min, the distillation temperature of the primary molecular distillation is 68-72 ℃, and the distillation temperature of the secondary molecular distillation is 108-112 ℃, the best bacteriostatic activity can be achieved for Propionibacterium acnes, and the stability is good. In addition, in the preparation method provided by the application, the microwave extraction power, the distillation pressure, the sample injection temperature, the condensation temperature and the feed rate of the primary molecular distillation, and the distillation pressure, the sample injection temperature, the condensation temperature and the feed rate of the secondary molecular distillation all have important influences. Among them, examples 1 to 4 are preferable examples in the present application.
Efficacy evaluation experiments:
first, experiment of melanin
Taking the cortex mori radicis extract prepared in example 1 as an example, the cortex mori radicis extract samples were diluted to concentrations of 0.625%, 0.3125%, 0.156%, 0.078%, respectively, and the melanocytes after administration were detected by an alkaline lysis method, and the melanocyte group without any treatment was a blank control group (BC), and the results are shown in table 2.
TABLE 2 change of melanin content by cortex Mori extract
As can be seen from table 2, different concentrations of cortex mori were all effective in reducing the concentration of melanin in the skin compared to the BC group, wherein the higher the concentration of cortex mori extract, the better the melanin lightening effect. Therefore, the cortex mori extract with the concentration in the listed range can be used for preparing the skin care product with the effects of whitening and lightening spots.
Second, Propionibacterium acnes inhibition experiment
Adding the final cortex Mori extract obtained in example 1 into Tryptone Soy Agar (TSA) culture medium (40-50 deg.C) sterilized under high pressure to obtain mixture with concentration of 50%, 25%, 12.5%, 6.25%, 3.125%, 0.625%, 0.125%, 0.025%, mixing agar and sample, pouring into flat dish, and mixing to obtain 1 × 108CFU/mL～2×108CFU/mL bacterial suspension according to 1: 10 dilution, 1 mu with sterile inoculating loopL bacterial suspension to growth control plate without sample, TSA plate surface with sample and second growth control plate. The final bacterial liquid inoculation amount is 104CFU/point, after culturing in an anaerobic jar at 36 ℃ for 72h, the bacteriostatic effect was evaluated, and the results are shown in Table 3.
TABLE 3 inhibitory effect of different concentrations of cortex Mori extract on Propionibacterium acnes growth
As can be seen from table 3, based on propionibacterium acnes, the Minimum Inhibitory Concentration (MIC) of the sample cortex mori radicis extract in the concentration range of 0.025% to 50% is 0.125%, and propionibacterium acnes are not detected in the rest 7 concentration experimental groups, which indicates that the cortex mori radicis extract prepared in the example has an obvious inhibition effect on the colony growth of propionibacterium acnes, and can effectively prevent the abnormal proliferation of propionibacterium acnes in sebum, thereby achieving the purpose of improving acne.
Third, experiment of antiseptic challenge
The preservative challenge test of the cortex mori radicis extract prepared in example 1 was performed using five kinds of microorganisms selected from staphylococcus aureus, pseudomonas aeruginosa, escherichia coli, candida albicans and aspergillus niger, and the total number of colonies in the petri dish was recorded on days 0, 7, 14 and 28 from the start of the test, respectively, and the results are shown in table 4.
TABLE 4 antiseptic challenge test results for cortex Mori extract
As can be seen from table 4, the cortex mori radicis extract prepared by the method has a good inhibition effect on the 5 microorganisms, and the cortex mori radicis extract meets the grade a standard required in the antibacterial protection evaluation standard ISO 11930-2019 of cosmetics, so that the cortex mori radicis extract can be applied to the cosmetics and has good preservative capability.
In summary, the preparation process of the cortex mori radicis extract provided by the application adopts traditional Chinese medicine plant sources, has the advantages of more active ingredients, simple process flow and recyclable solvent, and can be used for industrial production. And through tests, the obtained product can show better whitening and bacteriostasis effects and has good stability; the obtained product can effectively lighten melanin in skin, has good antiseptic capability while inhibiting abnormal reproduction of propionibacterium acnes, can simultaneously realize the effects of improving acne, lightening spots, whitening and brightening skin, and provides a theoretical basis for the use of the product in related-effect cosmetics.
The above description is only an example of the present application and is not intended to limit the present application. Various modifications and changes may occur to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the scope of the claims of the present application.
Claims (10)
1. A preparation method of a cortex mori extract for whitening and bacteriostasis is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: heating and refluxing the cortex mori radicis by using ethanol with the mass concentration of 70-90% for 3-4 hours at the temperature of 70-90 ℃ for primary ethanol extraction to obtain a cortex mori radicis primary ethanol extract, decoloring and filtering to obtain a cortex mori radicis filtrate;
step two: sequentially carrying out primary molecular distillation and secondary molecular distillation on the cortex mori radicis filtrate, and merging light fractions obtained by molecular distillation to obtain cortex mori radicis molecular distillate;
step three: performing vacuum filtration on the cortex mori molecular distillate by using diatomite cake, performing secondary alcohol extraction to obtain a cortex mori secondary alcohol extract, and performing rotary evaporation and concentration to obtain a cortex mori concentrate;
step four: pretreating the cortex mori radicis concentrate, carrying out vacuum filtration, adding 1, 3-propylene glycol to compound to the full weight of the pretreated cortex mori radicis concentrate, and obtaining the cortex mori radicis extract.
2. The method for preparing the cortex mori radicis extract for whitening and bacteriostasis as claimed in claim 1, wherein in the second step, the primary molecular distillation and the secondary molecular distillation are carried out under the assistance of microwave, the microwave power is 100-300W, and the distillation extraction time is 40-100 min.
3. The preparation method of the cortex mori extract for whitening and bacteriostasis according to claim 1, which is characterized by comprising the following steps: in the second step, the first step is carried out,
the conditions of the first-stage molecular distillation are as follows: the distillation pressure is 0.1-10 Pa, the sample injection temperature is 40-50 ℃, the distillation temperature is 50-80 ℃, and the condensation temperature is 20-40 ℃;
the conditions of the secondary molecular distillation are as follows: the distillation pressure is 0.1-10 Pa, the injection port temperature is 50-70 ℃, the distillation temperature is 100-120 ℃, and the condensation temperature is 60-70 ℃.
4. The preparation method of the cortex mori radicis extract for whitening and bacteriostasis according to claim 1, wherein in the first step, the amount of ethanol is 6-10 times of the mass of the cortex mori radicis.
5. The preparation method of the cortex mori radicis extract for whitening and bacteriostasis according to claim 1, characterized in that in the first step, activated carbon is adopted for decolorization, and the specific steps are as follows: heating in a water bath at 70-90 ℃ for 30-60 min, and filtering to remove the active carbon while the solution is hot.
6. The method for preparing the cortex mori radicis extract for whitening and bacteriostasis according to claim 1, wherein in the third step, the diatomite cake is prepared by adopting diatomite and EDTA-2Na, the dosage of the diatomite is 1% -10% of the molecular distillation mass of the cortex mori radicis, and the dosage of the EDTA-2Na is 0.2% -5% of the molecular distillation mass of the cortex mori radicis.
7. The method for preparing the cortex mori radicis extract for whitening and bacteriostasis according to claim 1, wherein in the third step, the molecular distillate of the cortex mori radicis needs to be cooled to 50-70 ℃ before vacuum filtration; and or (b) a,
the secondary alcohol extraction adopts absolute ethyl alcohol as an extractant, and the heating reflux is carried out for 3 to 4 hours at the temperature of 70 to 90 ℃; and or (b) a,
the rotary evaporation concentration conditions are as follows: the vacuum degree is 100-200 mbar, and the water bath temperature is 70-80 ℃.
8. The method for preparing the whitening and bacteriostatic cortex mori radicis extract according to claim 1, wherein the pretreatment of the cortex mori radicis concentrate in the fourth step comprises the steps of fully dissolving 1-4% of the concentrate with 25-30% of deionized water and 66-74% of 1, 3-propylene glycol, adding 5-8% of diatomite, stirring for 2-4 hours, and standing overnight.
9. A cortex Mori extract prepared by the method of any one of claims 1-8.
10. Use of a white mulberry root-bark extract as claimed in claim 9 for the preparation of a preparation for inhibiting the growth of propionibacterium acnes and/or lightening the melanin of the skin.
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